CN106457199B - Mesoscopic stream control reactor with impulse ultrasound wave frequency rate - Google Patents
Mesoscopic stream control reactor with impulse ultrasound wave frequency rate Download PDFInfo
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- CN106457199B CN106457199B CN201580028576.1A CN201580028576A CN106457199B CN 106457199 B CN106457199 B CN 106457199B CN 201580028576 A CN201580028576 A CN 201580028576A CN 106457199 B CN106457199 B CN 106457199B
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- reactor
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- spray nozzle
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/002—Nozzle-type elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00119—Heat exchange inside a feeding nozzle or nozzle reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00159—Controlling the temperature controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The present invention relates to a kind of for executing the mesoscopic stream control reactor of the chemical reaction of raw material, wherein the Component composition of the reactor is together to form the reactor, the reactor has the pipeline (3) for being suitable for delivering the fluid in high-pressure fog head (4), and high-pressure fog head (4) is equipped with the piezoelectric crystal unit for generating ultrasonic wave and has nozzle.The fog-spray nozzle is configured to generate the particle diameter distribution with nanoscale and micron particles in the case where fluid phase starting material and generates the particle diameter distribution with nanoscale, micron order or even more large-size particle in the case where solid-phase raw materials.
Description
Technical field
The present invention relates to chemical reactors.Particularly, it is anti-for executing vacuum flash pyrolysis (VFP) that the present invention relates to one kind
The equipment for being embodied as mesoscopic stream control reactor answered, the equipment have ultrasonic atomization to reduce particle diameter distribution, that is, increase and set
Solution/solid reagent dispersion degree needed for the reaction occurred in standby together with inert gas/reagent gas feeding.
Background technique
Implement in a controlled manner at high temperature and pressure in the shortest possible time in past decades to preferably anti-
The sustainable growth of the demand for the reactor answered.Such reactor is especially because growing to rapid and low-level byproduct
The demand of generation and emerge in large numbers.
This causes a kind of novel scientific domain, is referred to as " flash chemistry " with english term.Implementation is fallen into this field
The reactor of reaction is so-called flash reactor.J.Yoshida et al. summarize the field most important feature (referring to
Flash Chemistry:Fast Chemical Synthesis by Using Microreactors；Chemistry–A
European Journal 14(25),pp.7450-7459,2008).One of such device is noteworthy characterized by can be by means of fast
The fast temperature control that speed feedback is realized, and efficient heat exchange and/or heat transmitting.Since reagent mixes in this reactor
The residence time of object is short, so these reactors are also able to carry out than conventional more selective reaction.
In order to execute chemical reaction, due to multiple, it is vital for selecting temperature.Firstly, chemical reaction rate
Improved by temperature (referring to for example well-known Arrhenius relationship-K.J.Laidler, Chemical Kinetics,
Third Edition(1997),Benjamin-Cummings).Secondly, in order to start to react, need largely be in by activation energy
The form of heat is transferred to reaction mixture.However, reaction temperature it is higher and/or participate in reaction compound (initial reactant,
Product, solvent, other auxiliary substances and additive) be exposed to high temperature time it is longer, what is occurred in reaction mixture is not intended to
The amount of some byproducts and decomposition product is mostly and higher.The further raising of temperature will also cause to reach reaction mixture
Boiling point, this is undesirable in the chemical reaction for example executed in continuous tubular reactor.Therefore, chemical anti-when to execute
At once, the reaction temperature for optimizing specific reaction is particularly important.
In analytics, atomization/atomization/be well-known the technology for being sent into sample by spraying, it is known that be largely used to reality
The now approach of the technology.Its earliest and most common form first is that pneumatic nebulization, in particular with high-speed gas (so-called combustion
Burn gas) concentric pneumatic nebulization.This is most often used in flame atomic absorption spectrometry, wherein import gas (such as
Air, oxygen) supply flame burning.However, in Conventional pneumatic atomizer, since excessive substance and gas stream will be put out
Plasma torch and problem occurs.In order to avoid such case, the flow of both sample and burning gases has been reduced.This has passed through
The internal diameter (0.2mm) for reducing the capillary of atomizer is realized.However, as a result, atomization effect is also sharply declined.In addition,
Due to the precipitating and subsequent blocking at capillary end, it is invalid that concentration by weight typically becomes higher than 1% solution.
Since quite non-uniform particle diameter distribution is presented in an obtained aerosol, so being mounted in front of atomizer
Spherical shape collision ontology.It is collided by the drop and the ontology that force an aerosol, the drop is further beaten
It is broken, while biggish drop is only captured.The secondary particulate obtained in this way is then together with conveying gas from concentrically
Baffle installing, being oriented radially passes through.As a result, biggish drop is captured again.The aerosol three times being achieved in that
Particle diameter distribution would be about 5 μm.
Ultrasonic atomization has been described as further improving atomization effect.Its core feature be using being suitable for and/or
The generator of the ultrasonic wave with the frequency fallen into the frequency range from 200kHz to 10MHz can be generated.Pass through generator
The wave that is formed at liquid/gas interface of oscillation cause aerosol to generate.Average particle size distribution caused by this way depends on wanting
The surface tension and density of the liquid of atomization and the frequency of ultrasound source.Ultrasonic ultrasonic delay line memory can be divided into two groups.Belonging to
In the case where one group of atomizer, solution is directed on chemically-resistant piezo-electric crystal, and in the case where another group, transfer is longitudinal
The medium of (or pressure) wave imports between solution and the piezo-electric crystal that can be vibrated.Compared with pneumatic nebulization, ultrasonic atomization draws
Play particle diameter distribution more evenly.In addition, the physical characteristic of drop can be controlled by changing the frequency of ultrasound source.
Spraying in coatings art, especially ultrasonic atomization is most frequently used as feasible technological means, wherein counting
Micron uniform layer thickness, reproducibility and productivity it is extremely important.When application is spraying, usually the surface of different geometries is applied
Add inorganic material.Similar technology is chemical vapor deposition (CVD), is also used for usually by under high temperature and in vacuum
Specific inorganic compound carrys out coating surface.
International publication volume No.WO2012/033786 discloses a kind of solution, and one or more of them evaporates apolar substance
It is imported into pyrolytic deposition system to form cadmium sulfide photovoltaic film.For this purpose, using including cadmium, sulphur and at least under dissolved state
A kind of solution of other selected substance.The other selected substance (ethyl alcohol) of the solution be it is nonpolar, evaporate to obtain ratio
Water is fast, but its ratio of heat capacities water is low.The mixture setting is including one or more fog-spray nozzles and one or more heating dresses
In the pyrolytic deposition system set.The deposit of desired layer on substrate, the substrate be with a distance from fog-spray nozzle it is adjustable and
Its temperature can be controlled by one or more heating devices.
According to the document, although implementing spraying/atomization method in pyrolytic deposition system, will not send out in this case
Raw organic chemical reactions, because used technique is substantially based on inorganic substances.In addition, will not change when the procedure is completed
Learn conversion.
U.S. publication volume No.US20030230819 teaches a kind of for that will have low point by means of ultrasonic ultrasonic delay line memory
The drug ingedient of son amount is fitted into the method in microcapsules.Used equipment includes coaxial atomizer, two liquid inlets and one
A supersonic generator.A kind of liquid flows through inner nozzle, and another liquid flows through outer nozzle.Two plumes are from same atomization face
Pass through, wherein mixture is broken into microlayer model due to vibrational energy.The particle diameter distribution being achieved in that between 1 to 100 μm it
Between.Therefore ultrasonic ultrasonic delay line memory will not damage biological substance with low-energy operation, such as blood, antibody and bacterium.
The process occurs at low temperature there are two hybrid systems, it is therefore intended that is applied effective component
It covers.Organic chemical reactions will not occur in the case where common for pyrolysis.In addition, using ultrasonic spray system
Realize best mixing and partial size；It does not both refer in the document or does not imply using ultrasonic atomization and improve chemical activity.
International publication volume No.WO2013/050402 report it is a kind of can manufacture it is organic comprising compound and catalyst
The equipment of metal --- being known as metal organic framework (MOF) ---.In general, using hydrothermal method, wherein crystal from thermometal (such as
Metal salt) solution slowly grows.It slowly and with reversible manner is grown with crystal, so wherein forming the probability of defect
It is high.In case of in this case, then crystal must dissolve again, this causes crystal to fall into millimeter and micron size range.
The document also discloses a kind of method, wherein by least one metal ion and at least one tool there are solvent
There is the organic ligand of divalent to be supplied in spray dryer.Mixture passes through from nozzle and the drop therefore formed passes through
Hot gas dispersion.As a result, the reaction time needed for synthesis substantially reduces, dry crystal is collected, and can avoid filtering and into one
The processing step of step.
This temperature that compared with pervious method there is the manufacturing method of the effect significantly improved only to cover 80 to 200 DEG C
Spend range.In addition, it is not suitable for ultrasonic atomization unit, because the purpose to be realized does not include that small particle size distribution and reaction are mixed
Close the reactive increase of object.
Also spray pyrolysis technologies are learnt from the application for disposing hazardous material.Particularly, United States Patent (USP) No.5,359,
947 teach that a kind of molten metal for by means of being heated to 800 DEG C destroys the danger of packaging and toxicity clinical waste is
System.The reactor includes two-part pyrolysis unit and leads to packaging from the first combustion chamber and be given to the second combustion chamber therein
The outlet at bottom for molten metal.The glassware that is melted on the surface of molten metal, corrosion resisting steel (such as injection needle
Material) and the dissolution of more metal objects, organic material burn and resolve into their ingredient.The path of thermal decomposition product is added
To 250 DEG C, and therefore, any pathogen and hazardous material are destroyed heat in the system.
In the case where waste destruction, it is not usually required to control complexity by means of changing temperature, flow and other parameters
Response path.It is thus impossible to which the use of the spray pyrolysis in the field is compared with technology described in detail below.
Summary of the invention
The purpose of the present invention
According to above-mentioned, it appears that spray technique is not commonly used for executing hot organic chemistry in general organic chemistry laboratory
Reaction.The finite availability of the especially described technology of its reason and immature.
According to the prior art, it should be apparent that, there is currently no can apply or not apply inert gas or examination
--- i.e. atomization/sprinkling --- dissolution and/or solid matter are sprayed in the case where agent gas and therefore are executed in pyrolysis system
The device of unimolecule and bimolecular reaction.
Therefore, the purpose of the present invention is to provide one kind have ultrasonic spray unit --- i.e. atomizer/be sprayed
Device --- equipment, be used to implement vacuum flash pyrolysis (VFP) reaction, and more particularly to the type flow control reactor.
In general, the room temperature mixture of initiating reagent is fed into flow control reactor by means of pump, the then mixing
Object is heated to suitable temperature in reactor, and desired chemical reaction occurs at the raised temperature and then reacts
Mixture is cooled and draws from reactor to be further processed.Flow control reactor is needed using high performance liquid chromatography method
(HPLC) generally well-known device and equipment in field, because HPCL device is also at elevated pressures and in continuous flowing
Manage a small amount of liquid.Therefore, the component identical or closely similar with the unit of HPLC device --- such as pump, pipeline, container, detection
Device etc. --- it can also be used in (micro-) flow control reactor.Correspondingly, flow control according to the present invention is reacted unless otherwise
Device is described, and otherwise from now on, term " HPLC device " refers to HPLC device known to those skilled in the art.For example,
It when referring to the pump of flow control reactor of the invention, describes unless otherwise, otherwise refers to HPLC well known in the prior art
Pump.
According to above-mentioned, utilize it is another object of the present invention to provide a kind of for substantially --- but be not unique
Ground --- implement the method for the equipment (from now on: VFP equipment) of VFP reaction, the method be suitable for about temperature and/or
Execute organic chemical reactions on the wider scale of pressure, preferably within the temperature range of extending to 1000 DEG C from room temperature and/or
From 10-3Mbar is extended in the pressure limit of 400bar.
Yet another object of the invention is that developing a kind of flow control reactor, it is able to carry out VFP reaction and is preferred
Continuous flowing and Lab Scale reactor as mesoscopic stream control reactor.
Yet another object of the invention is that constructing a kind of for device and method of the invention and particularly for above-mentioned
Spraying (atomization) device of the flow control reactor of invention, one side can provide on demand uniform in the spraying generation of solution
Particle diameter distribution falls into the particle diameter distribution in nanometer and micron size range, and on the other hand can be applied not only to atomized soln, and
And it is also applied for that indissoluble or insoluble solid matter is made to enter thermal response.
Above-mentioned purpose is realized by mesoscopic stream control reactor according to claim 1.It is explained in claim 2 to 15
State the further preferred embodiment of the reactor.
Particularly, on the one hand, the purpose of the present invention is realized by a kind of continuous flow reactor, and the continuous flowing is anti-
Answering device includes heat-insulated multi-portion heating unit, reactor tube, for conveying raw material (liquid), inert gas/reagent gas pipe
Road and HPLC pump, the control valve for controlling inert gas/reagent gas direction, for measuring and controlling inert gas/examination
The mass flowmenter of agent gas, pressure gauge are obtained for the container (or solids container) of store solids material, for collecting conversion
The product collector of material, using for realizing vacuum and vacuum pump (for measuring and controlling the unit of vacuum degree)
Vacuum interface and equipped with generate ultrasonic wave piezoelectric crystal unit and nozzle high-pressure fog head.
More specifically, a kind of multifunctional equipment has been developed, wherein the raw material to be converted are in given vacuum degree and certain temperature
Degree is lower to enter gas phase/vapor phase (that is, specifically, evaporation and/or distillation).The product utilization VFP equipment obtained in conversion exists
It is condensed in preheated zone, the time of contact in the VFP equipment and passing through big energy barrier in milliseconds is at high temperature
Promote chemical conversion.VFP system is generally used for unimolecule conversion, this is because the average free road in the case where applying vacuum
Diameter is typically facilitated to inner molecular reaction.Ultrasonic atomization module (or it can be also known as to pneumatic spray module sometimes) is also formed
A part of multifunctional equipment according to the present invention；It is held in the module also with feeding inert gas/reagent gas
Row bimolecular (intramolecular) chemical reaction.
In addition, also achieving the high pressure (400bar) and height for executing heterogeneous catalysis, bimolecular and multiphase chemical process
Warm (600 DEG C) module.
Particularly, developed a kind of ultrasonic wave VFP equipment of tool there are three module, the device extension be related to from room temperature to
1000 DEG C of temperature and it is related to from 10-3The range of the suitable parameters of the pressure of mbar to 400bar.
Equipped with the ultrasonic atomization of a part for forming the VFP equipment of the invention implemented as mesoscopic stream control reactor
The pneumatic spray module of head with by the inert gas at a temperature of being in 1000 DEG C and/or other reagent gas by that can be fed into
The unit for being atomized both liquid-phase reagent solution and solid matter in equipment in combination provides.Therefore the module is suitable for making non-
Volatile materials enters reaction, and implements bimolecular and homogenous catalyst reaction with liquid phase and vapor phase.With regard to HPLC pump, pipeline
For internal diameter and flowing property, the feeding of raw material is fallen into micro-fluidic mechanism.Therefore used pneumatic spray module has
The advantages of can tracking well and the quantity of material in reaction volume is imported according to flow and concentration calculation unit time.
The pneumatic spray module for forming a part of VFP equipment of the invention for being embodied as mesoscopic stream control reactor is also suitble to
The indissoluble or insoluble material of solid state are in atomization.Due to the electrically driven (operated) piezoelectricity of one or more of pneumatic fog-spray nozzle
The Mechanical Moving of crystal, the solid particulate materials with greater particle size (for example, micron, millimeter) are broken.It can be by being applied
The tranmitting frequency of piezo-electric crystal change the intensity of the mechanical movement.One or more of piezo-electric crystal generations can also be used for wrapping
The heat of the heat demand of distillation containing solid matter.The solid matter smashed in this way is holding while being given in reaction volume
The compensator or trimmer pressure of 0.2-0.3bar is maintained in device, wherein the change of desired/plan occurs while it passes through from reaction volume
Learn transformation/conversion.
The basis of successful conversion is, with high-speed from the pneumatic fog-spray nozzle of the ultrasonic sprayer equipped with preferred design
The molecule left is further speeded up by carrier gas and is therefore only reacted in several milliseconds (ms) in high-temperature reactor.Guidance
Substance and increase and decrease --- i.e. control --- its residence time, which preferably pass through, to be applied vacuum and adjusts imported carrier gas/reagent gas
Flow realize.Due to the extremely short residence time, substance to be reacted is not exposed to thermally decompose.Preferably mesoscopic stream control reacts
The VFP equipment of the invention with ultrasonic atomization of device operates in wide parameter area and expands feasible chemical reaction
Range.The ultrasonic atomization list of inert gas/reagent gas changeability with high atomization effect and importing of the equipment
Member allows to execute further types of reaction.
By ultrasonic atomization unit, the solution with low concentration or middle concentration can be handled.Equipment according to the present invention is suitable
Solid material is guided to pass through ultrasonic atomization head together in together with application inert gas/reagent gas or vacuum.
In our study, we have obtained unexpected conclusion, that is, even if the particle of micron and non-nano size
Into reaction, high response is also presented in the substance of non-vaporising.
According to above-mentioned, the VFP equipment for being embodied as mesoscopic stream control reactor has following favorable characteristics:
It is suitable for implementing within several milliseconds of residence time within the temperature range of room temperature is to 1000 DEG C unimolecule and double
Molecule reaction, and the inert gas imported along the direction that the helical flow specified material of the wall of reactor tube flows and prevents material
Collision between reactor wall.
Its inside dimension (that is, diameter of its cylinder-shaped flow section) is fallen into from several millimeters to the size range of about 1cm,
And it wherein can also be so that ultrasound source provides thermal energy needed for making the solid matter distillation and makes importing later
Gas/vacuum guides the object that indissoluble or insoluble solid matter is made also to enter reaction by way of reaction volume.
In addition to inert gas, flow that can also be known and controlled imports other reagent gas wherein as carrier gas.
Fog-spray nozzle allows uniform particle diameter distribution (20 μm of >) in conjunction with ultrasound unit and pneumatic unit.
The waste heat of the ultrasound unit of fog-spray nozzle is preferred for the gas that preheating imports, therefore ultrasound unit is used
The heat exchanger for acting on input gas facilitates the cooling for maintaining the temperature of reaction zone and preventing its unexpected.
Product obtained is collected in the product collector/product condenser for the formula of suitably cooling, and the cooling is excellent
Choosing is by means of the mixture of dry ice and acetone or by being filled with the mixture, the cooling device of liquid nitrogen or other solvents, Po Er
Paste element (Peltier element), quencher, reflux cooler or any other type known to those skilled in the art
Heat exchanger realize.The product collector also may make up water-cooling apparatus.
The flow of the solution of changeable raw material, technical construction are insensitive to the type of solvent.
The atomisation pressure of the solution of raw material is in the range of being depressed into 400bar from atmosphere.
The heating of the reaction volume (preferred reactor pipe 12) of reactor includes the area of at least three separate detections and control
T1、T2、T3.The different temperatures in the furnace area is provided by the next door specially designed thus.
The heating of reactor tube in equipment is based on the subregion (zone by zone) for allowing the total length along reactor tube
Uniform temperature distribution indirect heating principle.The structure allows quickish temperature to adjust, and therefore it prevents reaction mixed
It closes and forms unfavorable temperature gradient in object.
Detailed description of the invention
Below with reference to attached drawing, the present invention will be described in detail, in the accompanying drawings
- Fig. 1 shows the one of the VFP equipment according to the present invention for being embodied as mesoscopic stream control reactor in schematic sectional view
A preferred illustrative embodiment；
- Fig. 2 shows one for the pneumatic spray module in VFP equipment according to the present invention in schematic sectional view
Possible exemplary embodiment；And
- Fig. 3 A and 3B are shown with curve mode and form for being embodied as the sight stream that is situated between by according to the present invention respectively
Control the 6 π electrocyclic reaction of Gould-Jacobs that the VFP equipment of reactor executes (its more detail is described about example 1)
The separation yield depending on fluid flow and ultrasonic frequency.
Specific embodiment
The VFP equipment according to the present invention for being preferably implemented as high temperature mesoscopic stream control reactor is shown in FIG. 1.According to Fig. 1,
The component of equipment of the invention --- according to its two kinds of different operation modes (i) and (ii) (i.e. respectively solution and/or solid material
The atomization of material) --- it connects as follows.
(i) in the container 1, the container 1 is optionally and in case of need through being suitble to for the setting of (liquid phase) raw material
It is connect in the pipeline 3 that pump 2, the preferably HPLC of conveying liquid pumped and were suitable for conveying liquid with high-pressure fog head 4 (referring to fig. 2),
Spray of the high-pressure fog head equipped with piezoelectric crystal unit (it preferably emits in ultrasonic wave range) and with spray tip
Mouth, the spray tip have the internal diameter of preferred 0.5mm, more preferable 0.2mm and most preferably from about 0.1mm.Raw material are to by spraying
Occur to warp let-off pipeline 3 optionally with the aid of pump operation 2 in first 4.Fog-spray nozzle 4 is through pipeline 10 and inert gas and other reagents
The gas source 6 of gas connects, wherein the gas source 6 (generates gas by for example one or more cylinders or gas generator on the spot
Body) or combinations thereof provide.In the inert gas and other reagent gas for being limited by pipeline 10 and being guided into from gas source 6 fog-spray nozzle 5
Flow path in, be provided with control valve 7, mass flowmenter 8 and pressure gauge 9 in succession in gas flow direction.Fog-spray nozzle 4 with
Sealing means are connect with the approaching side of the reactor tube 12 of the preferred tubulose of equipment according to the present invention.In order to be adjusted on demand by institute
The temperature for the reaction volume that reactor tube 12 is limited/surrounded is stated, whole length of the reactor tube 12 are configured in heating unit
In 11.The discharge side of reactor tube 12, which is led to, to be obtained for conversion cooling and that therefore condensation/precipitating leaves thermal response volume
In the product collector 13 of the cooled of substance.Finally, the outlet of vacuum interface 14 and vacuum pump 15 and product collector 13 connects
It connects.
(ii) inert gas and other reagent gas from gas source 6 through control valve 7, mass flowmenter 8 and pressure gauge 9 via
The pipeline 10 enters solids container 5, and in this case, solids container 5 accommodates solid-phase raw materials；Here, the solids container 5
It is connected directly to fog-spray nozzle 4 from below at a generally normal anglely.In addition, fog-spray nozzle 4 and the approaching side of reactor tube 12 are directly connected to.
Whole length of the reactor tube 12 configure in heating unit 11.It is similar to operation mode (i), the discharge of reactor tube 12
The production of the cooled for substance cooling and that therefore condensation/precipitating is obtained from the conversion that the reactor tube 12 leaves is led in side
In product collector 13.In addition, vacuum interface 14 and vacuum pump 15 are connect with the outlet of product collector 13.
Reactor tube 12 --- average diameter of the reaction volume defined by the reactor tube 12 --- is at least
10mm, preferably at least 15mm or more, and its length can arbitrarily select in the range of extending to 2000mm from 10mm.Reaction
One of the bigger internal diameter of volume between multiple reactor tubes parallel to each other the advantage is that optionally, can separate.
This means that more than one reactor tube 12 can be arranged in simultaneously in heating unit 11.In this case, naturally, in basis
The approaching side and discharge side of chemical mesoscopic stream control reactor 100 of the invention need to modify (about such as sprayer unit or product
The quantity and arrangement/connection of collector).The reactor tube 12 is preferably by from borosilicate, quartz, high silica glass, corrosion-resistant
The material selected in the group of steel and Hastelloy material is made.
For collecting the product collector 13 of substance that conversion obtains preferably with the high surface area condenser of precooling or molten
The form of agent absorber provides.Inert gas/reagent gas can be any one of hydrogen, nitrogen, oxygen etc..Mass flow
Meter 8, control valve 7 and pressure gauge 9 are for controlling inert gas/reagent gas pressure and flowing.In order to guide the flowing of substance
And the residence time is reduced, using vacuum pump 15.Equipment belongs to micro-fluidic range for feeding those of fluid phase starting material component
(for their relevant parameter).The feeding of solid-phase raw materials passes through suitable and known approach/hand by the solids container 5
Duan Zhihang.
The pneumatic of ultrasonic atomization head with the VFP equipment according to the present invention for being embodied as mesoscopic stream control reactor is sprayed
The structure of module is shown in FIG. 2.
On the one hand ultrasonic atomization head 4 for being embodied as in the VFP equipment of the invention of mesoscopic stream control reactor includes
It communicates with each other through material container 8 ' and on the other hand warp for conveying inert gas/reagent gas insulated gas pipeline 15 '
Atomizer 19 and ultrasound unit 25.
Liquid phase and/or solid-phase raw materials are provided in the material container 8 '.Ultrasound unit 25 includes one (optional
Ground is more than one) piezo-electric crystal 1 '.In order to receive the volume change occurred due to machine work, at least one described piezo crystals
Body 1 ' is covered with padding 2 '.In order to guarantee chemical resistance, piezo-electric crystal 1 ' is covered with ceramic wafer 3 ' with the surface of starting material.
The ultrasound unit 25 of equipment according to the present invention also serves as heat exchanger.For this purpose, being covered with the piezo-electric crystal 1 ' of the padding 2 '
It is entangled in the form of tubular big envelope by the aluminium block 26 with equally spaced groove 4 ', wherein groove 4 ' is formed in described piece and deviates from
The side (i.e. the outside of block 26) of piezo-electric crystal 1 '.In order to provide air-tightness, groove 4 ' is covered on the surface for being pushed against aluminium block
Polymer/PTFE seal set 5 '.The outer surface of sealing shroud 5 ' is by also ensuring that is be achieved in that is used as heat exchange in operation
Entangles and support to the fitting aluminium of the pressure thight of the unit of device/6 ' tubular of steel casing.Inert gas/reagent gas via
The gas access 7 ' of the unit and gas through the unit enter interconnecting piece 13 ' into ultrasound unit 25.In this way, indifferent gas
Body/reagent gas, which enters, enters the groove 4 ' that interconnecting piece 13 ' is connected to gas.Here, the preheating of inert gas/reagent gas is logical
It crosses and occurs to flow into preheat using the heat (it is unfavorable to reaction in some cases) generated during the operation of piezo-electric crystal 1 '
Inert gas/reagent gas；The inert gas of inflow/reagent gas is flowed along the groove 4 ' preferably spirally formed, thus
Absorb the heat generated by the piezo-electric crystal 1 ' and heating.Next, inert gas/the reagent gas is through ultrasound unit 25
Gas discharge interconnecting piece 14 ' leave, by gas pipeline 15 ' and then enter atomization through connection and thermometer mounting blocks 17
Device 19.The gas preheating can also be defeated the gas of the diameter of suitable (actually small) made of suitable structural material
It send in pipe insertion groove 4 ' and realizes.Here, it should also consider being remarkably decreased for heat transfer efficiency.
Atomizer 19 is by preferably from corrosion resisting steel, quartz, borosilicate, high silica glass, Hastelloy material, PEEK material
It is made with the structural material selected in the group of polytetrafluoroethylene (PTFE) (Teflon).
Inert gas/reagent gas forms vacuum by capillary 20 formed in atomizer 19 with high-speed.This
The vacuum that sample generates extends and leads to the mother tube 9 ' in material container 8 ' from described via being approximately perpendicular to 20 ground of capillary
Material container 8 ' suction by ultrasound unit 25 be broken into small particles and/or by the table in piezo-electric crystal 1 ' and ceramic wafer 3 '
The heat generated on face and the small size particle substance to distil.The vacuum is then by the way that particulate matter to be sprayed/be atomised in stream
Tomorrow, reactor tube 12 conveyed the particulate matter, and wherein reactor tube 12 connects along sealing ring 21 and atomizer 19 in a gastight manner
It connects.In order to improve nebulization efficiency, in the case where solution, solution is subjected at least one pressure as described in the ultrasound unit 25
The dynamic mechanically impact that transistor applies.Drop leaves the surface of solution as a result, enters in movement and then towards capillary
20 conveyings, and the vacuum then formed in the mother tube 9 ' and due to the flowing of inert gas/reagent gas are towards reaction
Device pipe 12 conveys.
Material container 8 ' is connect through threaded joints 12 ' with atomizer 19.In order to avoid distillation precipitation of material in cold spot
On, the interconnecting piece is entangled by tempering set 23.If too small by means of the heat that pre- hot inert gas/reagent gas dissipates,
The tempering set 23 can be cooled on the outside.Therefore, can simply avoid due to the heat that generates when piezo-electric crystal 1 ' operates and
Evaporation of the solution of generation from the surface of ceramic wafer 3 '.Temperature in material container 8 ' is opened by being conducted through thermal element assembly
Mouth 10 ' is simultaneously sealed in the measurement of the thermometer 11 ' on material container 8 ' using suitable sealing ring.
Based on the thermometric temperature being sealed in by sealed part 18 in the connection and thermometer assembling block 17
Data also control inertia by means of insulation/pipeline heating part 16 before the inert gas/reagent gas enters atomizer 19
Gas/reagent gas temperature.In order to ensure inert gas/reagent gas of preferred temperature reaches atomizer 19, the gas
The compensation of heat loss and the additional heating of gas occurred in the gas pipeline 15 ' according to the temperature data of measurement.As a result, can
Reduce the temperature gradient across reaction volume in the inlet point of the reaction volume.
Piezo-electric crystal 1 ' is continuously powered, or is electrically connected instead by the voltage of the type matching with the piezo-electric crystal
Part 24 is periodically powered.When ultrasound unit 25 is activated, it is once only capable of operating within the scope of single frequency.Piezo crystals
Body 1 ' is formed as replaceable units, therefore can be replaced according to the frequency to be realized.It is specific by applying to the piezo-electric crystal
Voltage and activate, wherein the voltage pass through square-wave signal modulate.According to the duty ratio of square-wave signal, sound wave will be continuous
Or dynamic pulse.
The VFP equipment for being embodied as mesoscopic stream control reactor with ultrasonic atomization head may be essentially available for two applications
In field: (i) is so that mode of the waste heat for pre- hot inert gas/reagent gas is atomized with the small particle under micron system
The solution of distribution, and (ii) atomization/distillation indissoluble or insoluble solid.However, aobvious and easy to those skilled in the art
See, this equipment can not also substantially change its structural intergrity and therefore without departing from the guarantor of following following claims
It is used in the other application field different from application field defined above in the case where protecting range.
In operation mode (i), the solution of raw material enters ultrasonic atomization head 4 from below, by pump 2 or due to literary mound
In principle and conveyed.Solution under the pressure that the resistance due to system accumulates through diameter be about 0.2mm pipe/capillary into
Enter reactor tube.Inert gas/reagent gas is fed into system along the entire periphery of the capillary, this reduces and dispersion
Into the size of the drop of reaction volume.In order to be further reduced the particle diameter distribution of the drop, ultrasonic atomization head 4 is with can be
(operation) the frequency operation freely changed between 500kHz and 5MHz；In this way, controlling fogging degree.Generate the electrification of ultrasonic wave
(live) piezoelectric unit generates heat during operation.The waste heat be used for preheat importing inert gas/reagent gas so as to reduce by
The temperature gradient caused by the gas of inflow.In order to realize good heat transfer, such as by keeping the element direct or indirect
It contacts and establishes mechanical attachment between the piezo-electric crystal utilized and pipe/pipe coil (coil)；The mediate contact is for example
By means of being embedded between the piezo-electric crystal and the coil of the pipe/pipe there is the material of thermal conductive resin to realize.In this way,
Ensure the expectation heating degree of gas.
In operation mode (ii), by means of inert gas/reagent gas through valve 7 and the importing of pressure gauge 9 under
Side is connected to the compensator or trimmer pressure for generating and maintaining about 0.2-0.3bar in the solids container 5 of ultrasonic atomization head 4.By utilizing pressure
The mechanical work of transistor, particle diameter distribution reduce to 100 to 250 μm of range from the range of millimeter range and/or hundreds of microns.This
Sample, on the one hand, it is processed that the substance can be used as process flows (i.e. fine powdered material), and on the other hand, the table of piezo-electric crystal
The heat generated on face induces the distillation of the substance；The gaseous material being achieved in that is then by the indifferent gas of offer compensator or trimmer pressure
Body/reagent gas is carried and is flowed into reaction volume.
The heating for the reactor tube 12 being heated is by indirect heating (for example, by infrared heating, cartridge heater, heating
Silk, heat blow etc.) it provides；Therefore, room temperature (here, about 20 DEG C to 25 DEG C) and at least about 1000 can be realized in reaction volume
Any temperature between DEG C.The reaction volume being heated is surrounded by the multilevel insulator with low heat transfer coefficient.Including more
The temperature of the furnace of a individual reaction zone is by least one temperature-sensing device of each area, preferably by the way that furnace chamber is arranged in
Temperature sensor measurement in given area.
The reactor tube 12 for being heated to the mesoscopic stream control size range of high temperature is arranged along its whole length in heating unit
In 11, wherein the ultrasonic atomization head 4 is located at approaching side, and the precooling of species precipitate/condensable product collector 13 is big
Surface area is located at the discharge side of the heating unit 11.
Optionally, vacuum pump 15 is for guiding material stream and being further reduced the residence time；The vacuum pump 15 can be borrowed
Help for example suitable pipeline to connect with the outlet of species precipitate/condensable product collector 13.
One of the VFP equipment for being embodied as mesoscopic stream control reactor with ultrasonic spraying device according to the present invention is excellent
The exemplary embodiment of choosing has following unrestricted technical parameter:
Temperature range: between room temperature (i.e. about 20 DEG C to 25 DEG C) and 1000 DEG C；
Temperature controlled precision: at 100 DEG C or less ± 3%, and at 100 DEG C or more ± 2% and 1000 DEG C or less ± 2%；
Nominal pressure: 10-3Between mbar and 3bar；
Inert gas/reagent gas flow: 1 to 10000ml/min；
The flow of solution: 0.1 to 1000ml/min；
The pressure of solution: between about 1bar (atmospheric pressure) and 400bar；
The ultrasonic frequency of application: between 500kHz and 5MHz；And
Reactor size: 500x26mm.
It discusses and is executed in the chemical reactor equipped with ultrasonic spraying device according to the present invention in further detail below
Some chemical reactions and related measurement result.It is readily apparent that the chemistry is anti-for those skilled in the art
Device is answered to be also suitable for implementing other chemical reactions in the case where being suitably transformed (for such as pressure, temperature).
Therefore, the chemical reaction of following discussion should only be counted as not limiting the example of the application range of chemical reactor of the invention.
Embodiment
6 π electrocyclic reaction of embodiment 1:Gould-Jacobs.
6 π electrocyclization of the Gould-Jacobs experiment executed in vacuum flash pyrolysis (VFP) device
The measuring raw materials of 200mg amount are supplied in the cucurbit of device.Then, by the temperature control unit of preheater
It is set as 150 DEG C, and the temperature control unit of reactor is set as 450 DEG C.Set value realization and stablize it
Afterwards, 10 are formd in systems-3The vacuum of mbar.Due to the temperature and vacuum, raw material start distillation and the several seconds exists later
Be precooled to -78 DEG C and occur in the product collector that configured in the exit for the reactor tube that length is 500mm from anti-
The product for answering device to obtain.Product obtained is dissolved by ethyl alcohol and/or methylene chloride from collector, and is then evaporated.Such as
It is necessary to product receives further purification to fruit.
6 π electrocyclization of the Gould-Jacobs experiment executed in ultrasonic vacuum flashing speed oven (UVFP) device
The measuring raw materials of 1390mg amount are supplied in cucurbit, and then in the dimethyl acetamide of 50ml
(DMA) dissolution in.In this way, obtaining the solution of the concentration with 0.1M.The temperature control unit of reactor is set as 450 DEG C.
It is 0.5ml/min by the flow set of solution, nitrogen flow is set as 2l/min, and the frequency of ultrasound unit is set
For 1.7MHz.After pumping the flowing several seconds for starting solution by HPLC, it is being pre-cooled to -78 DEG C of high surface area product
Occurs the product to be collected in collector.As long as the solution of raw material is used up in inlet, product is arranged from the collector
Out and evaporate.If it is necessary, product receives further processing.
Fig. 3 A and 3B are shown with curve mode and form be embodied as mesoscopic stream control reaction according to the present invention respectively
The separation of the flow for depending on application in the case where the VFP equipment of device and the 6 π electrocyclic reaction of Gould-Jacobs of frequency
Yield.When optimization (simplex method), only fluid flow and ultrasonic frequency change；All other parameter remains unchanged.It is obtained
The measurement result obtained clearly illustrates, such as the application of ultrasonic wave plays reaction process in the case where above-mentioned chemical reaction
Effect of optimization, that is, can make to separate yield maximization in the case where application ultrasonic wave.
Embodiment 2:Conrad-Limpach cyclization.
The Conrand-Limpach cyclisation experiment executed in vacuum flash pyrolysis (VFP) device
The measuring raw materials of 200mg amount are supplied in the cucurbit of device.Then, by the temperature control unit of preheater
It is set as 150 DEG C, and the temperature control unit of reactor is set as 450 DEG C.Set value realization and stablize it
Afterwards, 10 are formd in systems-3The vacuum of mbar.Due to the temperature and vacuum, raw material start distillation and the several seconds exists later
Be precooled to -78 DEG C and occur in the product collector that configured in the exit for the reactor tube that length is 500mm from anti-
The product for answering device to obtain.Product obtained is dissolved by ethyl alcohol and/or methylene chloride from collector, and is then evaporated.Such as
It is necessary to product receives further purification to fruit.
The Conrand-Limpach cyclisation experiment executed in ultrasonic vacuum flashing speed oven (UVFP) device
The measuring raw materials of 1050mg amount are supplied in cucurbit, and then in the dimethyl acetamide of 50ml
(DMA) dissolution in.In this way, obtaining the solution of the concentration with 0.1M.The temperature control unit of reactor is set as 450 DEG C.
It is 0.4ml/min by the flow set of solution, nitrogen flow is set as 2l/min, and the frequency of ultrasound unit is set
For 2.0MHz.After pumping the flowing several seconds for starting solution by HPLC, it is being pre-cooled to -78 DEG C of high surface area product
Occurs the product to be collected in collector.As long as the solution of raw material is used up in inlet, product is arranged from the collector
Out and evaporate.If it is necessary, product receives further processing.
According to this teaching, it will be readily apparent to one skilled in the art that according to the present invention be preferably implemented as being situated between
The ultrasonic wave VFP equipment for seeing flow control reactor, which is also suitable for executing, reacts different chemical reactions from VFP.
Claims (26)
1. it is a kind of for executing the mesoscopic stream control reactor of the chemical reaction of raw material, wherein the component of the reactor is according to institute
The phase for stating raw material is grouped together to form the reactor according to one of following scheme, and the reactor includes:
(i) in the case where fluid phase starting material,
Store the container (1) of the fluid phase starting material；
Equipped with the piezoelectric crystal unit for generating ultrasonic wave and with the high-pressure fog head (4) of nozzle；
The pipeline (3) of fluid communication is provided between the container (1) and the fog-spray nozzle (4)；
Reactor tube (12) with entrance and exit；
Accommodate the heating unit of the reactor tube (12), wherein
The fog-spray nozzle (4) is connected to the entrance of the reactor tube (12)；
The outlet of the reactor tube (12) is connected to collects to the product for the cooled for collecting the substance from chemical reaction
Device (13)；With
The product collector (13) has the outlet for being connected to vacuum interface (14) and vacuum pump (15), to be conducive to vacuum
It uses；
It provides inert gas/reagent gas gas source (6)；
Gas connection is provided between the gas source (6) and the fog-spray nozzle (4) the inertia of the gas source (6) will be come from
Gas/reagent gas feeds the gas pipeline (10) into the fog-spray nozzle (4), wherein control valve (7), mass flowmenter (8)
It is sequentially inserted into the gas pipeline (10) with pressure gauge (9), or
(ii) in the case where solid-phase raw materials,
Store the solids container (5) of the solid-phase raw materials；
Equipped with the piezoelectric crystal unit for generating ultrasonic wave and with the high-pressure fog head (4) of nozzle, wherein the solids container
(5) it is connected to the fog-spray nozzle (4) from below at a generally normal anglely；
Reactor tube (12) with entrance and exit；
The heating unit of the reactor tube (12) is accommodated,
The fog-spray nozzle (4) is connected to the entrance of the reactor tube (12)；
The outlet of the reactor tube (12) is connected to the product collector of the cooled to collect the substance that conversion obtains
(13)；With
The product collector (13) has the outlet for being connected to vacuum interface (14) and vacuum pump (15), to be conducive to vacuum
It uses；
It provides inert gas/reagent gas gas source (6)；
Gas connection is provided between the gas source (6) and the solids container (5) the lazy of the gas source (6) will be come from
Property gas/reagent gas through the solids container (5) feed gas pipeline (10) into the fog-spray nozzle (4), wherein control
Valve (7), mass flowmenter (8) and pressure gauge (9) are sequentially inserted into the gas pipeline (10),
It is characterized in that,
The heating unit is arranged to heat-insulated multi-portion heating unit (11)；
The fog-spray nozzle (4) is configured to generate the partial size point with nanoscale and micron particles in the case where fluid phase starting material
Cloth and particle diameter distribution of the generation with nanoscale, micron order or even more large-size particle in the case where solid-phase raw materials；
And wherein the gas pipeline (10) is arranged to add by the waste heat generated by the piezoelectric crystal unit in use
Heat, so that preheating flows through the inert gas/reagent gas of the gas pipeline (10).
2. reactor according to claim 1, which is characterized in that the fog-spray nozzle (4) further includes as the nozzle
Atomizer (19) and with the atomizer (19) in conjunction with as described in generate ultrasonic wave piezoelectric crystal unit ultrasonic wave list
First (25) form material container (8 ') between the atomizer (19) and the ultrasound unit (25), the atomizer
It (19) include the capillary (20) having a first end and a second end, the first end of the capillary (20) is formed by the nozzle,
The material container (8 ') is connected to the capillary (20) and the ultrasound unit (25), wherein the ultrasound unit
(25) include tubular big envelope to entangle the block of the piezoelectric crystal unit (26) form, wherein on the tubular big envelope
It is formed with the spiral groove (4 ') of hermetic seal, the spiral groove (4 ') is configured to provide the gas pipeline (10) and institute
The gas connection between the second end of capillary (20) is stated so that the inert gas/flow of reagent gases can be made in use
It is dynamic to pass through.
3. reactor according to claim 1 or 2, which is characterized in that the fog-spray nozzle (4) is configured to through the nozzle
Spray tip is atomized the insoluble solid of solvent, solution and distillation under stress, and the internal diameter of the spray tip, which is selected from, includes
The group of 0.5mm, 0.2mm and 0.1mm.
4. reactor according to claim 1 or 2, which is characterized in that the piezoelectric crystal unit includes in replaceable list
At least one piezo-electric crystal (1 ') of n-ary form n is so that the piezoelectric crystal unit can be grasped under various different frequencies as needed
Make.
5. reactor according to claim 1 or 2, which is characterized in that HPLC pump or other pumps (2) for conveying liquid
It is inserted between the container (1) and the fog-spray nozzle (4) in the pipeline (3).
6. reactor according to claim 2, which is characterized in that the atomizer (19) is by from corrosion resisting steel, quartz, boron
Silicate, high silica glass, Hastelloy material, PEEK material and Teflon group in the structural material that selects be made.
7. reactor according to claim 1 or 2, which is characterized in that the raw material are with solid fines end shape substance
Form is placed in the solids container (5).
8. reactor according to claim 1 or 2, which is characterized in that the average diameter of the reactor tube (12) is extremely
Few 10mm.
9. reactor according to claim 1 or 2, which is characterized in that be provided in the heating unit (11) mutually
The more than one reactor tube (12) extended parallel to.
10. reactor according to claim 9, which is characterized in that each reactor tube (12) by from borosilicate,
Quartz, high silica glass, corrosion resisting steel and Hastelloy material group in the material that selects be made.
11. reactor according to claim 1 or 2, which is characterized in that the length of each reactor tube (12) is fallen into
Between 10mm to 2000mm.
12. reactor according to claim 1 or 2, which is characterized in that each reactor tube (12) be configured to by
It is emptied in vacuum pump (15) to execute chemical reaction and control residence time under a reduced pressure.
13. reactor according to claim 1 or 2, which is characterized in that the reactor configuration is at being allowed for the original
The variable nebulisation time of the solution of material.
14. reactor according to claim 1 or 2, which is characterized in that the product collector (13) or product condenser
Be set as in Water cooling type cooling device or be filled with the mixture of dry ice and acetone, the cooling device of liquid nitrogen, reflux cooler,
The form of Peltier element or the heat exchanger of any other type.
15. reactor according to claim 1 or 2, which is characterized in that heating unit (11) construction Composition Region provides
It is arranged in the indirect heating of each of described heating unit (11) reactor tube (12).
16. reactor according to claim 1 or 2, which is characterized in that it is described generate ultrasonic wave piezoelectric crystal unit by
It is applied to the square-wave signal modulation voltage driving of the unit.
17. reactor according to claim 1 or 2, which is characterized in that the piezo-electric crystal list of the fog-spray nozzle (4)
It is operated under the frequency that member freely can be changed between 500kHz to 5MHz.
18. reactor according to claim 1 or 2, which is characterized in that the reactor tube (12) or each reactor tube
(12) it is connected to the fog-spray nozzle (4) or the respectively nozzle of fog-spray nozzle (4) in a gastight manner.
19. reactor according to claim 10, which is characterized in that the length of each reactor tube (12) is in 10mm
To 2000mm.
20. reactor according to claim 10, which is characterized in that each reactor tube (12) be configured to by means of
Vacuum pump (15) empties to execute chemical reaction and control residence time under a reduced pressure.
21. reactor according to claim 10, which is characterized in that the reactor configuration is at being allowed for the former material
The variable nebulisation time of the solution of material.
22. reactor according to claim 10, which is characterized in that the product collector (13) or product condenser are set
It is set in Water cooling type cooling device or is filled with the mixture of dry ice and acetone, the cooling device of liquid nitrogen, reflux cooler, amber
You paste the form of the heat exchanger of element or any other type.
23. reactor according to claim 10, which is characterized in that heating unit (11) construction Composition Region provides cloth
Set the indirect heating in each of described heating unit (11) reactor tube (12).
24. reactor according to claim 10, which is characterized in that the piezoelectric crystal unit for generating ultrasonic wave is by applying
Add to the square-wave signal modulation voltage driving of the unit.
25. reactor according to claim 10, which is characterized in that the piezoelectric crystal unit of the fog-spray nozzle (4)
It is operated under the frequency that freely can be changed between 500kHz to 5MHz.
26. reactor according to claim 10, which is characterized in that the reactor tube (12) or each reactor tube
(12) it is connected to the fog-spray nozzle (4) or the respectively nozzle of fog-spray nozzle (4) in a gastight manner.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| HU1400180A HUP1400180A2 (en) | 2014-03-31 | 2014-03-31 | Pulsating audio frequency mesofluidic reactor |
| HUP1400180 | 2014-03-31 | ||
| PCT/HU2015/000031 WO2015150845A2 (en) | 2014-03-31 | 2015-03-31 | Mesofluidic reactor with pulsing ultrasound frequency |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106457199A CN106457199A (en) | 2017-02-22 |
| CN106457199B true CN106457199B (en) | 2019-04-30 |
Family
ID=89991461
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201580028576.1A Expired - Fee Related CN106457199B (en) | 2014-03-31 | 2015-03-31 | Mesoscopic stream control reactor with impulse ultrasound wave frequency rate |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US9901897B2 (en) |
| EP (1) | EP3126041A2 (en) |
| JP (1) | JP2017519631A (en) |
| CN (1) | CN106457199B (en) |
| HU (1) | HUP1400180A2 (en) |
| WO (1) | WO2015150845A2 (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5671648B1 (en) * | 2014-08-08 | 2015-02-18 | 黒崎播磨株式会社 | Thermal spray material |
| US10190058B2 (en) * | 2016-08-22 | 2019-01-29 | The University Of Toledo | High-yield production of fuels and petro- and oleo-chemical precursors from vegetable oils and other liquid feedstocks in a continuous-flow pyrolysis reactor with or without catalysts |
| CN110944743A (en) * | 2017-05-23 | 2020-03-31 | 生捷科技控股公司 | System and method for chemical synthesis on wafer |
| CN107555698B (en) * | 2017-10-26 | 2023-04-07 | 上海辨洁环保科技有限公司 | Rapid evaporation system and method for high-concentration concentrated solution |
| CN108853702B (en) * | 2018-05-15 | 2021-02-26 | 中国科学院苏州生物医学工程技术研究所 | Novel intelligent medicine sprinkling system |
| DE102018212411A1 (en) * | 2018-07-25 | 2020-01-30 | Robert Bosch Gmbh | Method for obtaining a breath sample from a test subject and device |
| CN110449310B (en) * | 2019-08-01 | 2021-07-16 | 南通市联缘染业有限公司 | Ultrasonic atomization auxiliary device and method for preparing antistatic polyester cotton yarn in auxiliary mode |
| CN111135770B (en) * | 2019-12-31 | 2022-06-24 | 河海大学常州校区 | Experimental research device and method for generation characteristics of catalytic synergistic discharge active ingredients |
| CN111905671A (en) * | 2020-07-16 | 2020-11-10 | 深圳石墨烯创新中心有限公司 | Corrosion-resistant ultrasonic reaction kettle |
| US11572324B1 (en) | 2021-09-09 | 2023-02-07 | Chevron Phillips Chemical Company, Lp | Methods for operating ethylene oligomerization reactor systems with an integrated ultrasonic flow meter |
| CN115739852A (en) * | 2022-10-27 | 2023-03-07 | 中核武汉核电运行技术股份有限公司 | Ultrasonic impact loosening device for hard sludge between heat transfer tubes of steam generator |
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- 2015-03-31 JP JP2017503193A patent/JP2017519631A/en not_active Ceased
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2015150845A3 (en) | 2016-01-28 |
| HUP1400180A2 (en) | 2015-10-28 |
| CN106457199A (en) | 2017-02-22 |
| US9901897B2 (en) | 2018-02-27 |
| US20170021328A1 (en) | 2017-01-26 |
| WO2015150845A2 (en) | 2015-10-08 |
| JP2017519631A (en) | 2017-07-20 |
| EP3126041A2 (en) | 2017-02-08 |
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